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A practical and innovative approach leading to structurally stable and tribologically effective polyurea grease via pre‐form thickener
2020 NLGI Virtual Technical WeekAugust 24 – 28, 2020
Presenter: Liwen Wei
Innovation in Grease : PU Pre‐form Thickener• PUG is a non‐metallic grease with soap like structures, known for its high temperature stability, low noise characteristic, good mechanical, oxidation and high‐shear stability, OEM and users’ first choice for premium grease ideal for sealed‐for‐life bearings, ball bearing, electric motors applications, and many more
• PU grease in‐situ manufacturing must deal with toxic MDI/TDI and hazardous amines ‐ Hamper development & difficult for small‐medium (and new) players
• This Study provides insights into making high performance polyurea grease via pre‐form powder with ease and flexibility
Slide 2
PU Grease: Opportunities & Challenges• PU grease, 6% market share globally, 29% share in Japan, is the best option to replace Lithium (65‐75% market share)
• PU grease in‐situ manufacturing must deal with toxic MDI/TDI and hazardous amines ‐ Hamper development & difficult for small‐medium (and new) players
Slide 3
Polyurea & Soap Thickeners are similar, made to form extensive H‐Bond Infrastructures
Lithium: Fibers(Metal base and 12‐HSA)
Polyurea: Platelets to Fibers (Urea/ [polyurea based)
OBCSC: Spherical (Calcite)
Slide 4
Isocyanate Mono and poly amine
MDI Aliphatic & Alicyclic
MDI Aromatic
TDI Aliphatic & Alicyclic
Polyurea Thickeners have much higher H‐bond Forming Tendency with higher Melting Point than Soap Thickeners
Slide 5
PUG = PUT Powder + Oils + Additives Specialty Additive (SA)
• A: S/P Inorganic + DMTD + FM• B: Ashless Sulfur (Inactive) + DTC• C: B + S/P Inorganic + FM• D: DTC + DMTD + FM
Synthetic Base Oil (SBO)• AN 23: Alkylated Naphthalene• PAG 320: Water Insoluble PAG• HSE 320: Biodegradable Complex Ester• DC 220: Di‐capped PAG
Slide 6
Stage Two Oil Back, Mill to #2 PUG
Stage One Maximize PUT Gelling
Base Oil‐1 Base Oil‐2
Stage One: Shear Thickening Process (Masterbatch Production)Stage Two: Oil back to desire grease grade (Blending Operation)
PUT to PUG Conversion
Slide 7
FTIR: PUT‐made PUG versus In‐situ Commercial
PUG
Slide 8
FTIR: PUT‐made PUG in Various Synthetic Base
Oils
Slide 9
Post Process Milling is Vital to give structurally stable PUG
5000.00
10000.00
15000.00
20000.00
0 1800 3600 5400 7200
Time (Sec)
Vis
cosi
ty (
cP)
Not milledPartially Milled Fully Milled
Slide 10
Sample PUT Process SBO %
Powder#
Milling P0 P60 P10,000 Oil Sep (100C, 24h)
Dropping Point, C
PUG6 2‐Step AN23 10% 2 278 281 372 0.52% 248
PUG6 2‐Step AN23 10% 4 267 258 308 (P100K)
0.31% 250
PUG6 2‐Step AN23 9% 5 270 269 287 0.76% 246
PUG6 2‐Step AN23 7% 6 274 269 270 0.71% 232
PUG9 2‐Step AN23 11% 2 254 261 294 N/A 276
PUG10 2‐Step AN23 11% 2 269 303 350 N/A 283
Slide 11
Grease ID Penetration P50K D1831160C/12h
Dropping Point C
P# Delta P# Delta P#Full cup/cone Half cup/cone Half cup/cone
PUG (In Situ) 279 10 ‐2 315
PUG1 (PUT) 253 8 11 290
PUGA (In Situ) 276 23 140 252
PUGB (In Situ) 269 6 10 308
Slide 12
Polyurea Grease for Extreme Lubrication
Steel Mill Industry Example
Challenges: Bearings experience high temperatures and loads under high speed or super low speedoperation, as well as environments contaminated with water and debris. (Sounds familiar with Wind turbine?)
Opportunities: PU Grease or OBCSG Grease? Must be Tribologically EffectiveTesting, testing, & Verification
Slide 14
Tribological Testing to Tackle Extreme Lubrication: Understanding StribeckCurve & Chemistry Dynamics
• Tribological Effective Solutions • https://en.wikipedia.org/wiki/Extreme_tribology
• Beyond the original machinery design specifications.
• Beyond the original machinery ambient parameters & application in challenging environmental conditions
• Beyond the original lubricant design specification.
Slide 15
Grease SBO (ISO)
Total Dosage
Add. Package
S/P Booster
Sulfur EP
DTC/ DMTD FM
PUG9 AN23 7% A x x xLi G AN23 5% B x xPUG9 AN23 5% B x xPUG9 AN23 7% C x x x xPUG9 AN23 7% D x x
Tribological Testing Summary
Slide 16
Grease SBO (ISO)
Total Dosage
Add. Package
S/P Booster
Sulfur EP
DTC/ DMTD FM 4‐Ball
WeldFalex Weld
Ball on Disc Wear
Pin on Disc Wear
4‐Ball AW
PUG9 AN23 7% A x x x 800+ 1750+ Nil Best 0.65LiG AN23 5% B x x 625+ 4500+
PUG9 AN23 5% B x x 315+ 1750+ High Worst 0.56PUG9 AN23 7% C x x x x 800+ 4500+ High Better 0.55PUG9 AN23 7% D x x 800+ 4500+ 0.60
Tribological Testing* Summary
Slide 17
*4‐ball Weld: ASTM D2596, 4‐Ball AW: ASTM D2266, Falex: ASTM D3233
Grease SBO (ISO)
Total Dosage
Add. Package
S/P Booster
Sulfur EP
DTC/ DMTD FM 4‐Ball
WeldFalex P&V
Ball on Disc Wear
Pin on Disc Wear
4‐Ball AW
PUG9 AN23 7% A x x x 800+ 1750+ Nil Best 0.65Li G AN23 5% B x x 625+ 4500+PUG9 AN23 5% B x x 315+ 1750+ High Worst 0.56PUG9 AN23 7% C x x x x 800+ 4500+ High Better 0.55PUG9 AN23 7% D x x 800+ 4500+ 0.60
Maximum EP Performance with Mitigating AW/FM Performance : A, C, &D
Slide 18
*4‐ball Weld: ASTM D2596, 4‐Ball AW: ASTM D2266, Falex: ASTM D3233
0
500
1000
1500
2000
2500
3000
3500
4000
4500
PUG 9‐AN23 PUG 9‐E320 PUG 9‐G320 PUG 9‐DC220 CommercialPUG‐5%B
PUG 9‐5%B CommercialPUG‐5% S/P
PUG 9‐5%A PUG 9‐5%C
+ 5% B+ 5% B
+ 5% C+ 5% A
+ 5% S/P
+ E320+AN23 + G‐320 +DC‐220
Falex P&V is highly repeatable(Line Contact, Variable Load Stages)
Slide 19
Grease SBO (ISO)
Total Dosage
Add. Package
S/P Booster
Sulfur EP
DTC/ DMTD FM 4‐Ball
WeldFalex P&V
Ball on Disc Wear
Pin on Disc Wear
4‐Ball AW
PUG9 AN23 7% A x x x 800+ 1750+ Nil Best 0.65Li G AN23 5% B x x 625+ 4500+PUG9 AN23 5% B x x 315+ 1750+ High Worst 0.56PUG9 AN23 7% C x x x x 800+ 4500+ High Better 0.55PUG9 AN23 7% D x x 800+ 4500+ 0.60
4-Ball AW is not effective(Point contact, fixed Load/Speed)
*4‐ball Weld: ASTM D2596, 4‐Ball AW: ASTM D2266, Falex: ASTM D3233
Slide 20
Ball‐on‐Disc: Wear/COF/Wear Tracks
Ball on Disc (Point Contact/Rotating)
Rotary Speed: 16 stages/30s to 4,000RPMForce: 100N Constant
Slide 21
Ball‐on‐Disc Wear Scars
Effectively Ranks Base
Oils and Additives
Additive A: EP with AW/FM Additive B: S‐EP Additive C: S‐EP with S/P Booster
Base Oil 1 ‐ Polyalkylene Glycol Base Oil 2 – Alkylated Naphthalene Base Oil 3 ‐ High Stability Ester
Slide 22
Pin on Disc Picks the Winner A
• Pin On Disc • (Area Contact/Rotating)• Step One: 100N @50RPM• Step Two: 250N @500RPM
Slide 23
Conclusion (I):
PUG made via Pre‐Form
Thickener is a Premium High Temperature
Grease
• Organic Thickener: Inherently Structurally Stable and Environmentally Friendly
• Dropping Points: 2600C‐300+0C
• Outstanding High Temperature Mechanical Stability (160C@D1831)
Slide 24
Conclusion (II):
PUG is Tribologically Effective with
EP/Load Carrying& Mitigating AW/FM
Performance
• Explore use of Special Additives and Synthetic Base Oils
• Achieved 800+Kg 4‐ball Weld & 4500#+ Falex P&V load
• Ball on Disc and Pin on Disc offer Clear ranking of formulated Polyurea grease
Slide 25
Thank you & NLGI
Acknowledgement• John Blalock• Steven Mayorga• Jamie Blalock• Argentina Martinez
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